+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04src0951_90 started at 11:40:44 on 16-Dec-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src0951_295 in R-3m CELL 0.71073 7.3003 7.3003 17.2160 90.000 90.000 120.000 ZERR 3.00 0.0010 0.0010 0.0030 0.000 0.000 0.000 LATT 3 SYMM - Y, X - Y, Z SYMM - X + Y, - X, Z SYMM Y, X, - Z SYMM - X, - X + Y, - Z SYMM X - Y, - Y, - Z SFAC H FE K O S UNIT 18 9 3 42 6 V = 794.59 F(000) = 741.0 Mu = 4.92 mm-1 Cell Wt = 1502.45 Rho = 3.140 MERG 2 OMIT -3.00 55.00 OMIT -2 2 5 EXTI 0.00233 FMAP 2 PLAN 10 SIZE 0.05 0.05 0.05 ACTA WGHT 0.06600 5.14490 L.S. 6 TEMP -183.00 FVAR 0.31010 FE1 2 0.333333 0.166667 0.166667 10.25000 0.00253 0.00287 = 0.00469 -0.00023 -0.00045 0.00127 S1 5 0.666667 0.333333 0.024276 10.16670 0.00243 0.00243 = 0.00339 0.00000 0.00000 0.00122 O1 4 0.126656 -0.126656 0.135286 10.50000 0.00439 0.00439 = 0.00773 -0.00129 0.00129 0.00288 AFIX 3 H1 1 0.173256 -0.173791 0.120076 10.50000 0.03001 AFIX 0 O2 4 0.445996 0.222998 0.053336 10.50000 0.00195 0.00509 = 0.00453 0.00087 0.00174 0.00098 O3 4 0.666667 0.333333 -0.060591 10.16670 0.00640 0.00640 = 0.00228 0.00000 0.00000 0.00320 K1 3 0.000000 0.000000 0.000000 10.08330 0.00827 0.00827 = 0.00580 0.00000 0.00000 0.00414 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for 04src0951_295 in R-3m H 0.320 FE 1.240 K 2.270 O 0.660 S 1.030 Fe1 - O1_$9 O1_$2 O1 O1_$7 O2 O2_$7 K1 K1_$13 S1 - O3 O2_$11 O2_$12 O2 O1 - Fe1_$4 Fe1 K1 O2 - S1 Fe1 K1 O3 - S1 K1 - O1_$2 O1_$8 O1 O1_$6 O1_$10 O1_$4 O2_$6 O2 O2_$10 O2_$2 O2_$4 O2_$8 Operators for generating equivalent atoms: $1 x-2/3, y-1/3, z-1/3 $2 -y, x-y, z $3 -y+1/3, x-y-1/3, z-1/3 $4 -x+y, -x, z $5 -x+y+1/3, -x+2/3, z-1/3 $6 -x, -y, -z $7 -x+2/3, -y+1/3, -z+1/3 $8 y, -x+y, -z $9 y+2/3, -x+y+1/3, -z+1/3 $10 x-y, x, -z $11 -y+1, x-y, z $12 -x+y+1, -x+1, z $13 x+2/3, y+1/3, z+1/3 7403 Reflections read, of which 4969 rejected -8 =< h =< 9, -9 =< k =< 9, -18 =< l =< 22, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -1 6 2 294.01 3.40 10 37.15 -3 4 8 93.92 2.84 14 15.59 2 Inconsistent equivalents 254 Unique reflections, of which 0 suppressed R(int) = 0.0417 R(sigma) = 0.0328 Friedel opposites merged Maximum memory for data reduction = 1401 / 4029 Special position constraints for Fe1 x = 0.3333 y = 0.1667 z = 0.1667 U13 = 2.0 * U23 U12 = 0.5 * U11 sof = 0.25000 Input constraints retained (at least in part) for sof Special position constraints for S1 x = 0.6667 y = 0.3333 U22 = 1.0 * U11 U23 = 0 U13 = 0 U12 = 0.5 * U11 sof = 0.16667 Input constraints retained (at least in part) for sof Special position constraints for O1 y = -1.0 * x + 0.0000 U22 = 1.0 * U11 U13 =-1.0 * U23 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for H1 y = -1.0 * x + 0.0000 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O2 y = 0.5 * x + 0.0000 U13 = 2.0 * U23 U12 = 0.5 * U11 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O3 x = 0.6667 y = 0.3333 U22 = 1.0 * U11 U23 = 0 U13 = 0 U12 = 0.5 * U11 sof = 0.16667 Input constraints retained (at least in part) for sof Special position constraints for K1 x = 0.0000 y = 0.0000 z = 0.0000 U22 = 1.0 * U11 U23 = 0 U13 = 0 U12 = 0.5 * U11 sof = 0.08333 Input constraints retained (at least in part) for sof Least-squares cycle 1 Maximum vector length = 511 Memory required = 1503 / 52043 wR2 = 0.1153 before cycle 1 for 254 data and 27 / 27 parameters GooF = S = 1.257; Restrained GooF = 1.257 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0660 * P )^2 + 5.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31123 0.00353 0.319 OSF 2 0.00290 0.00124 0.460 EXTI Mean shift/esd = 0.361 Maximum = 0.715 for U22 Fe1 Max. shift = 0.002 A for O3 Max. dU =-0.007 for H1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1503 / 52043 wR2 = 0.1142 before cycle 2 for 254 data and 27 / 27 parameters GooF = S = 1.237; Restrained GooF = 1.237 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0660 * P )^2 + 5.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31244 0.00354 0.344 OSF 2 0.00320 0.00127 0.238 EXTI Mean shift/esd = 0.147 Maximum = 0.344 for OSF Max. shift = 0.001 A for O3 Max. dU =-0.003 for H1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1503 / 52043 wR2 = 0.1140 before cycle 3 for 254 data and 27 / 27 parameters GooF = S = 1.234; Restrained GooF = 1.234 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0660 * P )^2 + 5.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31255 0.00356 0.030 OSF 2 0.00324 0.00130 0.033 EXTI Mean shift/esd = 0.010 Maximum = 0.033 for EXTI Max. shift = 0.000 A for O1 Max. dU = 0.000 for H1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1503 / 52043 wR2 = 0.1140 before cycle 4 for 254 data and 27 / 27 parameters GooF = S = 1.234; Restrained GooF = 1.234 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0660 * P )^2 + 5.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31256 0.00356 0.003 OSF 2 0.00325 0.00130 0.003 EXTI Mean shift/esd = 0.001 Maximum = 0.003 for x O2 Max. shift = 0.000 A for O2 Max. dU = 0.000 for H1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1503 / 52043 wR2 = 0.1141 before cycle 5 for 254 data and 27 / 27 parameters GooF = S = 1.234; Restrained GooF = 1.234 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0660 * P )^2 + 5.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31256 0.00356 0.000 OSF 2 0.00325 0.00130 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for EXTI Max. shift = 0.000 A for O1 Max. dU = 0.000 for H1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1503 / 52043 wR2 = 0.1140 before cycle 6 for 254 data and 27 / 27 parameters GooF = S = 1.234; Restrained GooF = 1.234 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0660 * P )^2 + 5.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31256 0.00356 0.000 OSF 2 0.00325 0.00130 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for O1 Max. dU = 0.000 for H1 Largest correlation matrix elements 0.780 U22 Fe1 / OSF 0.699 EXTI / OSF 0.532 U11 S1 / U11 Fe1 0.759 U12 O1 / U11 O1 0.685 U33 Fe1 / OSF 0.504 U11 K1 / OSF 0.722 U22 Fe1 / U11 Fe1 0.622 U11 S1 / U22 Fe1 0.710 U11 Fe1 / OSF 0.609 U11 S1 / OSF 04src0951_295 in R-3m ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Fe1 0.33333 0.16667 0.16667 0.25000 0.00317 0.00350 0.00533 -0.00022 -0.00044 0.00158 0.00403 0.00000 0.00000 0.00000 0.00000 0.00000 0.00069 0.00061 0.00071 0.00017 0.00034 0.00034 0.00054 S1 0.66667 0.33333 0.02428 0.16670 0.00300 0.00300 0.00434 0.00000 0.00000 0.00150 0.00345 0.00196 0.00000 0.00000 0.00011 0.00000 0.00076 0.00076 0.00103 0.00000 0.00000 0.00038 0.00060 O1 0.12676 -0.12676 0.13536 0.50000 0.00525 0.00525 0.00828 -0.00158 0.00158 0.00327 0.00597 0.00342 0.00033 0.00033 0.00020 0.00000 0.00129 0.00129 0.00172 0.00067 0.00067 0.00147 0.00083 H1 0.17336 -0.17326 0.12015 0.50000 0.02031 0.00000 0.02480 O2 0.44596 0.22298 0.05341 0.50000 0.00338 0.00590 0.00521 0.00077 0.00154 0.00169 0.00511 0.00675 0.00055 0.00027 0.00018 0.00000 0.00187 0.00127 0.00159 0.00059 0.00118 0.00093 0.00086 O3 0.66667 0.33333 -0.06076 0.16670 0.00750 0.00750 0.00333 0.00000 0.00000 0.00375 0.00611 0.00570 0.00000 0.00000 0.00033 0.00000 0.00181 0.00181 0.00273 0.00000 0.00000 0.00090 0.00125 K1 0.00000 0.00000 0.00000 0.08330 0.00897 0.00897 0.00642 0.00000 0.00000 0.00449 0.00812 0.00000 0.00000 0.00000 0.00000 0.00000 0.00091 0.00091 0.00124 0.00000 0.00000 0.00045 0.00069 Final Structure Factor Calculation for 04src0951_295 in R-3m Total number of l.s. parameters = 27 Maximum vector length = 511 Memory required = 1476 / 24017 wR2 = 0.1140 before cycle 7 for 254 data and 0 / 27 parameters GooF = S = 1.234; Restrained GooF = 1.234 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0660 * P )^2 + 5.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0349 for 232 Fo > 4sig(Fo) and 0.0383 for all 254 data wR2 = 0.1140, GooF = S = 1.234, Restrained GooF = 1.234 for all data Occupancy sum of asymmetric unit = 1.67 for non-hydrogen and 0.50 for hydrogen atoms Principal mean square atomic displacements U 0.0054 0.0036 0.0031 Fe1 0.0043 0.0030 0.0030 S1 0.0100 0.0057 0.0023 O1 0.0067 0.0061 0.0025 O2 0.0075 0.0075 0.0033 O3 0.0090 0.0090 0.0064 K1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.035 0.064 0.089 0.126 0.175 0.221 0.269 0.349 0.443 1.000 Number in group 28. 24. 25. 25. 25. 26. 25. 25. 26. 25. GooF 0.907 0.934 1.154 1.019 0.921 0.835 1.287 0.665 2.558 0.931 K 1.014 0.941 0.935 0.989 0.972 0.968 1.006 1.027 1.005 1.059 Resolution(A) 0.77 0.80 0.83 0.88 0.92 1.00 1.08 1.19 1.40 1.77 inf Number in group 26. 25. 26. 25. 27. 24. 25. 25. 26. 25. GooF 0.952 0.836 0.724 0.826 0.793 0.805 0.781 0.894 0.986 2.981 K 0.977 0.993 1.029 1.018 1.039 1.043 1.052 1.048 1.046 1.020 R1 0.055 0.055 0.031 0.032 0.030 0.034 0.030 0.030 0.027 0.059 Recommended weighting scheme: WGHT 0.0711 2.5417 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 0 0 3 4773.07 14473.24 10.06 0.388 5.74 -1 1 1 3906.15 6571.88 4.51 0.261 5.93 -1 3 2 2050.08 1512.24 3.07 0.125 2.30 -1 4 1 464.93 610.24 1.85 0.080 1.74 0 3 6 107.70 49.64 1.81 0.023 1.70 0 1 14 84.56 161.47 1.73 0.041 1.21 -4 6 17 2805.48 3480.66 1.66 0.190 0.77 -1 1 10 928.20 752.36 1.63 0.088 1.66 -3 3 15 1460.11 1738.53 1.53 0.134 1.01 -1 6 2 3020.65 3827.69 1.48 0.199 1.13 -5 6 16 563.14 744.85 1.46 0.088 0.78 -1 5 0 2750.56 2400.30 1.42 0.158 1.38 0 3 3 77464.05 69459.57 1.34 0.849 1.98 -4 5 18 596.89 751.05 1.33 0.088 0.79 -2 7 12 411.86 544.30 1.29 0.075 0.83 0 5 16 127.11 13.82 1.28 0.012 0.82 -1 7 1 1882.52 2170.74 1.28 0.150 0.96 0 1 2 12973.37 15285.08 1.27 0.398 5.10 -1 7 4 151.09 222.45 1.21 0.048 0.94 -1 5 12 144.16 198.06 1.21 0.045 0.99 0 1 8 551.98 656.21 1.20 0.083 2.04 -1 2 12 652.01 552.54 1.20 0.076 1.34 -1 6 11 593.30 713.89 1.19 0.086 0.92 -3 6 9 406.68 331.45 1.18 0.059 1.03 0 7 11 146.79 22.95 1.18 0.015 0.78 -3 8 7 1355.55 1676.66 1.14 0.132 0.85 -3 8 10 3748.48 4289.73 1.13 0.211 0.80 -6 8 10 12622.04 10997.53 1.12 0.338 0.78 -5 7 12 -58.26 3.61 1.11 0.006 0.83 -4 5 15 1142.55 1310.90 1.11 0.117 0.88 -2 4 0 103615.80 94682.84 1.11 0.992 1.83 0 2 10 104978.34 96286.49 1.10 1.000 1.51 0 7 5 954.27 1143.29 1.09 0.109 0.87 0 6 6 19034.36 17267.20 1.09 0.423 0.99 -2 2 2 11098.85 12113.36 1.04 0.355 2.97 -4 7 10 589.06 690.03 1.03 0.085 0.89 0 4 11 20450.90 18776.71 1.03 0.442 1.11 -1 5 6 436.33 350.83 1.03 0.060 1.24 -1 1 7 56889.86 52484.29 1.02 0.738 2.29 -1 2 0 6228.91 5693.56 1.01 0.243 3.65 -2 3 10 18.84 1.73 1.01 0.004 1.40 -1 4 16 986.90 1123.42 1.01 0.108 0.92 0 6 15 3426.19 3960.97 0.98 0.203 0.78 -3 4 20 144.66 281.88 0.98 0.054 0.77 0 3 0 342.60 289.08 0.97 0.055 2.11 -4 4 10 33058.30 30552.98 0.97 0.563 1.16 -7 7 1 661.38 562.12 0.96 0.076 0.90 -2 9 1 -103.20 14.36 0.96 0.012 0.77 -1 4 19 1408.46 1589.87 0.96 0.128 0.80 0 5 4 37.42 70.29 0.94 0.027 1.21 Bond lengths and angles Fe1 - Distance Angles O1_$9 1.9806 (0.0015) O1_$2 1.9806 (0.0015) 180.00 O1 1.9806 (0.0015) 91.01 (0.23) 88.99 (0.23) O1_$7 1.9807 (0.0015) 88.99 (0.23) 91.01 (0.23) 180.00 O2 2.0759 (0.0031) 91.69 (0.12) 88.31 (0.12) 88.31 (0.12) 91.69 (0.12) O2_$7 2.0759 (0.0031) 88.31 (0.12) 91.69 (0.12) 91.69 (0.12) 88.31 (0.12) 180.00 K1 3.5601 (0.0004) 127.57 (0.11) 52.44 (0.11) 52.44 (0.11) 127.56 (0.11) 56.36 (0.10) 123.64 (0.10) K1_$13 3.5601 (0.0004) 52.44 (0.11) 127.56 (0.11) 127.56 (0.11) 52.44 (0.11) 123.64 (0.10) 56.36 (0.10) 180.00 Fe1 - O1_$9 O1_$2 O1 O1_$7 O2 O2_$7 K1 S1 - Distance Angles O3 1.4641 (0.0062) O2_$11 1.4827 (0.0034) 109.76 (0.14) O2_$12 1.4827 (0.0034) 109.76 (0.14) 109.18 (0.14) O2 1.4827 (0.0034) 109.76 (0.14) 109.18 (0.14) 109.18 (0.14) S1 - O3 O2_$11 O2_$12 O1 - Distance Angles Fe1_$4 1.9806 (0.0015) Fe1 1.9806 (0.0015) 134.28 (0.20) K1 2.8284 (0.0038) 93.85 (0.12) 93.85 (0.12) O1 - Fe1_$4 Fe1 O2 - Distance Angles S1 1.4827 (0.0034) Fe1 2.0759 (0.0031) 129.83 (0.21) K1 2.9656 (0.0035) 142.17 (0.18) 88.00 (0.11) O2 - S1 Fe1 O3 - Distance Angles S1 1.4641 (0.0062) O3 - K1 - Distance Angles O1_$2 2.8284 (0.0038) O1_$8 2.8284 (0.0038) 180.00 (0.08) O1 2.8284 (0.0038) 58.78 (0.13) 121.22 (0.13) O1_$6 2.8284 (0.0038) 121.22 (0.13) 58.78 (0.13) 180.00 (0.12) O1_$10 2.8284 (0.0038) 121.22 (0.13) 58.78 (0.13) 121.22 (0.13) 58.78 (0.13) O1_$4 2.8284 (0.0038) 58.78 (0.13) 121.22 (0.13) 58.78 (0.13) 121.22 (0.13) 180.00 (0.19) O2_$6 2.9656 (0.0035) 121.66 (0.05) 58.34 (0.05) 121.66 (0.05) 58.34 (0.05) 106.46 (0.10) 73.54 (0.10) O2 2.9656 (0.0035) 58.34 (0.05) 121.66 (0.05) 58.34 (0.05) 121.66 (0.05) 73.54 (0.10) 106.46 (0.10) 180.00 (0.09) O2_$10 2.9656 (0.0035) 73.54 (0.10) 106.46 (0.10) 121.66 (0.05) 58.34 (0.05) 58.34 (0.05) 121.66 (0.05) 110.84 (0.06) O2_$2 2.9656 (0.0035) 58.34 (0.05) 121.66 (0.05) 106.46 (0.10) 73.54 (0.10) 121.66 (0.05) 58.34 (0.05) 69.16 (0.06) O2_$4 2.9656 (0.0035) 106.46 (0.10) 73.54 (0.10) 58.34 (0.05) 121.66 (0.05) 121.66 (0.05) 58.34 (0.05) 69.16 (0.06) O2_$8 2.9656 (0.0035) 121.66 (0.05) 58.34 (0.05) 73.54 (0.10) 106.46 (0.10) 58.34 (0.05) 121.66 (0.05) 110.84 (0.06) K1 - O1_$2 O1_$8 O1 O1_$6 O1_$10 O1_$4 O2_$6 FMAP and GRID set by program FMAP 2 3 20 GRID -0.980 -2 -2 0.980 2 2 R1 = 0.0376 for 254 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.47 at 0.0000 0.0000 0.0000 [ 0.00 A from K1 ] Deepest hole -0.90 at 0.6667 0.3333 0.1401 [ 1.89 A from O1 ] Mean = 0.00, Rms deviation from mean = 0.26 e/A^3, Highest memory used = 1594 / 13288 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5000 0.5000 0.0000 0.25000 0.05 1.06 2.07 O2 2.15 S1 2.35 O3 2.92 H1 Q2 1 0.1676 -0.1676 0.0312 0.50000 0.05 0.97 1.53 H1 1.62 O2 1.87 O1 2.16 O3 Q3 1 0.6667 0.3333 -0.1667 0.08333 0.05 0.84 1.82 O3 2.18 H1 2.67 O1 3.29 S1 Q4 1 0.7344 0.2656 -0.0407 0.50000 0.05 0.67 0.92 O3 1.41 S1 1.71 O2 1.80 H1 Q5 1 0.4077 0.2038 0.0191 0.50000 0.05 0.55 0.64 O2 1.64 S1 2.14 O3 2.43 H1 Q6 1 0.3647 0.1824 0.0674 0.50000 0.05 0.55 0.57 O2 1.72 FE1 2.05 S1 2.36 O1 Q7 1 0.8524 0.4262 -0.0223 0.50000 0.05 0.46 1.35 O3 1.42 S1 1.84 O2 2.44 H1 Q8 1 0.3307 0.0000 0.0000 0.50000 0.05 0.41 1.68 O2 2.40 H1 2.40 H1 2.41 K1 Q9 1 0.0000 0.1727 0.0000 0.50000 0.05 0.39 1.26 K1 2.06 O2 2.43 H1 2.47 O1 Q10 1 0.5583 0.4417 0.0347 0.50000 0.05 0.38 1.38 S1 1.42 O2 2.14 O3 2.78 O2 Shortest distances between peaks (including symmetry equivalents) 5 6 0.87 1 10 0.95 2 5 0.98 7 10 1.00 1 7 1.01 4 7 1.10 8 9 1.15 1 8 1.24 2 4 1.25 9 9 1.26 4 5 1.29 2 9 1.32 2 8 1.32 5 8 1.34 4 4 1.48 5 10 1.54 8 10 1.56 7 8 1.60 5 7 1.63 5 9 1.65 7 10 1.68 6 8 1.69 2 6 1.71 4 10 1.77 6 9 1.79 6 10 1.79 2 7 1.83 4 8 1.89 10 10 1.90 1 5 1.94 1 4 1.96 7 7 2.02 7 7 2.03 4 7 2.05 8 9 2.09 4 6 2.14 2 10 2.16 1 2 2.17 9 9 2.18 6 7 2.27 2 6 2.30 1 6 2.33 3 4 2.33 10 10 2.37 2 2 2.38 1 9 2.39 2 5 2.39 8 8 2.41 7 10 2.41 4 5 2.42 4 9 2.45 8 8 2.47 9 9 2.52 2 9 2.52 4 10 2.53 2 10 2.55 9 10 2.57 4 10 2.58 7 9 2.59 2 4 2.64 5 7 2.64 5 10 2.64 5 5 2.66 4 8 2.69 7 8 2.73 3 7 2.75 6 7 2.77 5 5 2.84 2 7 2.85 8 10 2.86 5 6 2.87 6 9 2.87 5 9 2.89 5 7 2.90 1 7 2.91 4 7 2.92 5 8 2.97 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.52: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.03: Structure factors and derivatives 0.00: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.02: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04src0951_90 finished at 11:40:44 Total CPU time: 0.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++